Titanium-zirconium cross-linking agent and preparation method thereof
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A technology of cross-linking agent, titanium and zirconium, applied in chemical instruments and methods, drilling composition, etc., can solve the problems of poor cross-linking and pick-hanging performance.
Pending Publication Date: 2022-04-08
昆山京昆油田化学科技有限公司
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The commonly used acidic crosslinking agent is organic zirconium crosslinking agent, but organic zirconium crosslinking agent is sensitive to pH value under acidic conditions, and it has better crosslinking performance only when the pH value of the use environment is around 3; when using The pH value of the environment is higher than 5.5, and the cross-linking hanging performance is obviously deteriorated
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[0038] The present invention also provides a preparation method of the titanium-zirconium crosslinking agent described in the above technical scheme, comprising the following steps:
[0039] mixing inorganic titanium, ligands and water to obtain a suspension;
[0040] The suspension is mixed with inorganic zirconium to perform a first coordination reaction, and then a protonic acid is added to perform a second coordination reaction to obtain the titanium-zirconium crosslinking agent.
[0041] The invention mixes inorganic titanium, ligands and water to obtain a suspension.
[0042] In the present invention, the mixing temperature of the inorganic titanium, ligands and water is preferably 20-40°C, more preferably 30-35°C; the mixing time of the inorganic titanium, ligands and water is preferably 1-3 hours. In the present invention, the mixing of the inorganic titanium, the ligand and water is preferably carried out under the condition of stirring. In the present invention, th...
Embodiment 1
[0050] Add 5g of titanium phosphate and 60mL of water into a 250mL three-necked flask, stir thoroughly, then add 10mL of diethanolamine (10.9g) into the three-necked flask for stirring, and at the same time raise the temperature of the water bath to 30°C and keep the temperature constant for 1h; add 3g of oxychloride Zirconium, react at 30°C for 2h, then add 3g of citric acid, react at 40°C for 2h, and obtain the titanium-zirconium crosslinking agent.
Embodiment 2
[0052] Take 5g of titanium sulfate and 60mL of water and add them to a 250mL three-necked flask, stir thoroughly, then add 5mL of 40wt% ammonium citrate solution and 10mL of triethanolamine (11.36g) to the three-necked flask and stir, while the temperature of the water bath is raised to 35°C. And keep the temperature for 1h; add 2g of zirconium sulfate, react at 40°C for 3h, then add 3mL of pure acetic acid, react at 35°C for 2h, and obtain the titanium-zirconium crosslinking agent.
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Abstract
The invention belongs to the technical field of cross-linking agent preparation, and provides a titanium-zirconium cross-linking agent and a preparation method thereof. The titanium-zirconium cross-linking agent provided by the invention is prepared from the following raw materials: inorganic titanium, a ligand, inorganic zirconium, protonic acid and water, the inorganic titanium comprises titanium phosphate and/or titanium sulfate; the ligand comprises one or more of diethanol amine, triethanolamine, ammonium citrate and sodium gluconate; the inorganic zirconium comprises zirconium oxychloride and/or zirconium sulfate. According to the titanium-zirconium cross-linking agent, the titanium cross-linking agent and the zirconium cross-linking agent are introduced at the same time, so that the titanium-zirconium cross-linking agent has the advantages of the titanium cross-linking agent and the zirconium cross-linking agent at the same time, and the pH application range of the titanium-zirconium cross-linking agent is widened; meanwhile, the titanium-zirconium cross-linking agent has excellent temperature resistance. In addition, through selection of inorganic titanium, inorganic zirconium and the ligand, generation of alcohol small molecular compounds in the preparation process is avoided, and the titanium-zirconium cross-linking agent is good in stability and environmentally friendly.
Description
technical field [0001] The invention relates to the technical field of crosslinking agent preparation, in particular to a titanium-zirconium crosslinking agent and a preparation method thereof. Background technique [0002] Acidic crosslinking agent is an important crosslinking agent in the field of oilfield fracturing. The commonly used acidic crosslinking agent is organic zirconium crosslinking agent, but organic zirconium crosslinking agent is sensitive to pH value under acidic conditions, and it has better crosslinking performance only when the pH value of the use environment is around 3; when using When the pH value of the environment is higher than 5.5, the cross-linking hanging performance will be obviously deteriorated. Contents of the invention [0003] In view of this, the object of the present invention is to provide a titanium-zirconium crosslinking agent and a preparation method thereof. The titanium-zirconium cross-linking agent of the present invention has...
Claims
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